Abstract

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The siliconmicroreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy.Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

We thank the Alexander von Humboldt Foundation (A.R.), the “Stiftung der Deutschen Wirtschaft” (S.B.), and the Helmholtz-Kolleg “Energy related catalysis” (G.H.) for grants and the BMBF-projects “X-ray microscopy” (No. 05K10VK1) and “Nanoscopy” (No. 05K13VK2) and the virtual institute VI-403 “In-situ Nano Imaging of Biological and Chemical Processes” for financial support. In particular, GeSiM (Gesellschaft fuer Silizium-Mikrosysteme GmbH) is gratefully acknowledged for fruitful discussions on the design and for producing the custom-designed microreactor and A. Jahn (TU Dresden) is acknowledged for the discussion on this gas phase reactor setup. In addition, we thank InfraTec for test IR thermography measurements with the microreactor as well as Renishaw and Dr. Hudson Carvalho for Raman spectroscopy. Finally, we are grateful for allocation of beamtimes at SuperXAS at PSI, SUL-X and TOPOTOMO at ANKA and thank Dr. Maarten Nachtegaal, Dr. Dmitry Doronkin, Dr. Angelica Cecilia, the SUL-X beamline staff Dr. Anna Zimina, Dr. Ralph Steininger, and Dr. Jörg Göttlicher, Andreas Gänzler, Dr. Thomas Sheppard, and Dr. Federico Benzi for their help during beamtime measurements and Jörg Finsterle for building the electronics.

[Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in or on a common substrate or of specific parts thereof; Manufacture of integrated circuit devices or of specific parts thereof, Manufacture or treatment of devices consisting of
a plurality of solid state components or integrated circuits formed in or on a common
substrate or of specific parts thereof; Manufacture of integrated circuit devices or of
specific parts thereof]

Abstract

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The siliconmicroreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy.Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.